Plastics - Polyamides - Determination of viscosity number (ISO 307:2003)

Kunststoffe - Polyamide - Bestimmung der Viskositätszahl (ISO 307:2003)

Diese Internationale Norm legt ein Verfahren zur Bestimmung der Viskositätszahl (auch als reduzierte Viskositätszahl bezeichnet) von verdünnten Polyamid-lösungen in bestimmten, festgelegten Lösemitteln fest.
Das Verfahren ist auf Polyamide mit den Bezeichnungen PA 46, PA 6, PA 66, PA 69, PA 610, PA 612, PA 11, PA 12, PA 6T und PA MXD6, wie in ISO 1847-1 definiert, und Copolyamide und sonstige Polyamide anwendbar, die unter den festgelegten Bedingungen in einem der festgelegten Lösemittel löslich sind.
Das Verfahren ist nicht auf Polyamide anwendbar, die durch anionische Polymerisation von Laktamen oder mit Vernetzungsmitteln hergestellt wurden; derartige Polyamide sind normalerweise in den vorgeschriebenen Lösemitteln unlöslich.
Im Allgemeinen müssen die Polyamidproben in den aufgeführten Lösemitteln vollständig löslich sein und die in ihnen enthaltenen Additive (z. B. Verstärkungsfasern, Flammschutzmittel und Modifikatoren) dürfen sich nicht störend auf die Viskositätsmessung auswirken. Das Verfahren kann jedoch für die Überwachung der Herstellung von Mischungen angewandt werden, die Additive enthalten, die sich störend auf die Viskositäts-messung auswirken. In solchen Fällen hat die jeweilige Mischung eine bestimmte, in einem festgelegten Lösemittel gemessene Viskositätszahl, die an sich nicht von einem Lösemittel auf ein anderes Lösemittel umgewandelt werden kann, außer durch ein bestimmtes, die Mischung betreffendes Verhältnis, und die nur für den Vergleich von Produkten geeignet ist.
Die Viskositätszahl wird nach dem in ISO 1628-1 festgelegten allgemeinen Verfahren unter Beachtung der in dieser Internationalen Norm festgelegten besonderen Bedingungen bestimmt.
Die Bestimmung der Viskositätszahl eines Polyamids ergibt ein Maß für die relative Molekülmasse des Polymers.

Plastiques - Polyamides - Détermination de l'indice de viscosité (ISO 307:2003)

Polimerni materiali - Poliamidi - Določanje števila viskoznosti (ISO 307:2003)

General Information

Status
Withdrawn
Publication Date
30-Nov-2003
Withdrawal Date
02-Jul-2007
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
02-Jul-2007
Due Date
25-Jul-2007
Completion Date
03-Jul-2007

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Plastics - Polyamides - Determination of viscosity number (ISO 307:2003)Plastiques - Polyamides - Détermination de l'indice de viscosité (ISO 307:2003)Kunststoffe - Polyamide - Bestimmung der Viskositätszahl (ISO 307:2003)Ta slovenski standard je istoveten z:EN ISO 307:2003SIST EN ISO 307:2003en83.080.20PlastomeriThermoplastic materialsICS:SIST EN ISO 307:20001DGRPHãþDSLOVENSKI
STANDARDSIST EN ISO 307:200301-december-2003

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN ISO 307August 2003ICS 83.080.20Supersedes EN ISO 307:1997English versionPlastics - Polyamides - Determination of viscosity number (ISO307:2003)Plastiques - Polyamides - Détermination de l'indice deviscosité (ISO 307:2003)Kunststoffe - Polyamide - Bestimmung der Viskositätszahl(ISO 307:2003)This European Standard was approved by CEN on 1 August 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 307:2003 E

2003-10-01ForewordThis document (EN ISO 307:2003) has been prepared by Technical Committee ISO/TC 61"Plastics" in collaboration with Technical Committee CEN/TC 249 "Plastics", the secretariat ofwhich is held by IBN.This European Standard shall be given the status of a national standard, either by publication ofan identical text or by endorsement, at the latest by February 2004, and conflicting nationalstandards shall be withdrawn at the latest by February 2004.This document supersedes EN ISO 307:1997.According to the CEN/CENELEC Internal Regulations, the national standards organizations ofthe following countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland andthe United Kingdom.Endorsement noticeThe text of ISO 307:2003 has been approved by CEN as EN ISO 307:2003 without anymodifications.NOTE
Normative references to International Standards are listed in Annex ZA (normative).

Reference numberISO 307:2003(E)© ISO 2003
INTERNATIONAL STANDARD ISO307Fourth edition2003-08-15Plastics — Polyamides — Determination of viscosity number Plastiques — Polyamides — Détermination de l'indice de viscosité

ISO 307:2003(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
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ISO 2003 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel.
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ii © ISO 2003 — All rights reserved

ISO 307:2003(E) © ISO 2003 — All rights reserved iii Contents Page Foreword.iv 1 Scope.1 2 Normative references.1 3 Terms and definitions.2 4 Principle.2 5 Reagents and materials.2 6 Apparatus.3 7 Preparation of test samples.4 8 Calculation of mass of test portion.5 9 Selection of solvent.6 10 Procedure.7 11 Expression of results.9 12 Repeatability and reproducibility.9 13 Relationship between the viscosity number determined in 96 % (by mass) sulfuric acid solution and viscosity number determined in various other solvents.9 14 Test report.18 Annex A (normative)
Determination of the concentration of commercial sulfuric acid [95 % (by mass) to 97 % (by mass)] and adjustment to 96 % (by mass).20

ISO 307:2003(E) iv © ISO 2003 — All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 307 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9, Thermoplastic materials. This fourth edition cancels and replaces the third edition (ISO 307:1994), which has been technically revised.

INTERNATIONAL STANDARD ISO 307:2003(E) © ISO 2003 — All rights reserved 1 Plastics — Polyamides — Determination of viscosity number 1 Scope This International Standard specifies a method for the determination of the viscosity number (also referred to as reduced viscosity) of dilute solutions of polyamides in certain specified solvents. The method is applicable to the polyamides designated PA 46, PA 6, PA 66, PA 69, PA 610, PA 612, PA 11, PA 12, PA 6T/66 and PA MXD6 as defined in ISO 1874-1, as well as to copolyamides and other polyamides that are soluble in one of the specified solvents under the specified conditions. The method is not applicable to polyamides produced by anionic polymerization of lactams or produced with crosslinking agents; such polyamides are normally insoluble in the specified solvents. In general, polyamide samples have to be completely soluble in the solvents mentioned, and the additives contained in them (e.g. reinforcement fibres, flame-retardants and modifiers) must not interfere with the viscosity measurement. However, the method can be used for production control of compounds containing additives which interfere with the viscosity measurement. In such cases, a particular compound in a particular solvent will have a specific viscosity number which, in principle, cannot be converted from one solvent to another except by means of a relationship specific to the compound concerned. Viscosity numbers converted in this way are only suitable for inter-product comparisons. The viscosity number is determined by the general procedure specified in ISO 1628-1, observing the particular conditions specified in this International Standard. The determination of the viscosity number of a polyamide provides a measure of the relative molecular mass of the polymer. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks ISO 1628-1:1998, Plastics — Determination of the viscosity of polymers in dilute solution using capillary viscometers — Part 1: General principles ISO 1874-1:1992, Plastics — Polyamide (PA) moulding and extrusion materials — Part 1: Designation ISO 3105:1994, Glass capillary kinematic viscometers — Specifications and operating instructions ISO 3451-4:1998, Plastics — Determination of ash — Part 4: Polyamides ISO 6427:1992, Plastics — Determination of matter extractable by organic solvents (conventional methods) ISO 15512:1999, Plastics — Determination of water content

ISO 307:2003(E) 2 © ISO 2003 — All rights reserved ASTM D 789-98, Standard Test Methods for Determination of Relative Viscosity and Moisture Content of Polyamide (PA) JIS K 6920-2:2000, Plastics — Polyamide (PA) moulding and extrusion materials — Part 2: Preparation of test specimens and determination of properties 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 1628-1 and the following apply. 3.1 viscosity number VN 〈of a polymer〉 the value given by the equation 01VN1cηη=−× (1) where η is the viscosity of a solution of the polymer in a specified solvent; η0 is the viscosity of the solvent, expressed in the same units as η; c is the concentration, in grams per millilitre, of the polymer in the solution. NOTE The viscosity number is usually expressed in millilitres per gram. 4 Principle The times of flow of a solvent and a solution of the polyamide at a concentration of 0,005 g/ml in the solvent are measured at 25 °C, the same viscometer being used for both measurements. The viscosity number is calculated from these measurements and from the known concentration of the solution. 5 Reagents and materials Use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. WARNING — Avoid contact with the skin and inhalation of any vapours of the solvents and cleaning liquids. 5.1 Solvents 5.1.1 Sulfuric acid, (96 ± 0,15) % (by mass) solution. For the determination of the concentration of commercial sulfuric acid [95 % (by mass) to 97 % (by mass)] and adjustment to 96,0 % (by mass), see Annex A. 5.1.2 Formic acid, (90 ± 0,15) % (by mass) solution. The solvent shall be stored in a brown glass bottle. Its concentration shall be checked at least every 2 weeks. It shall not contain more than 0,2 % (by mass) of acetic acid or methyl formate.

ISO 307:2003(E) © ISO 2003 — All rights reserved 3 5.1.3 m-Cresol, meeting the following specifications: appearance: clear and
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